Method and apparatus for synthesizing lead β-diketonates

Abstract

A method and apparatus for the synthesis of β-diketonates such as Pb(fod) 2 and Pb(thd) 2 for use as precursors in metalorganic chemical vapor deposition processes. Lead oxide and a medium of pentane and a protonated ligand (H-fod or H-thd) are combined in a flask and subjected to reaction-promoting ultrasonic waves. The flask is immersed in a water bath to maintain a constant cool temperature, and the flask may include one or more arms for cooling and circulation of the medium during the reaction.

What is claimed is: 
     
       1. A method of producing a lead β-diketonate, comprising: combining lead oxide with a medium; subjecting the combined lead oxide and medium to ultrasonic waves, and recovering said lead β-diketonate. 
     
     
       2. The method of claim 1, further comprising: heating the medium in a vacuum to vaporize non-β-diketonate compounds in the medium. 
     
     
       3. The method of claim 1, wherein the lead oxide and medium are combined in a flask, and the step of subjecting the combined lead oxide and medium to ultrasonic waves is by placing an ultrasonic probe into the flask. 
     
     
       4. The method of claim 3, wherein the flask has a lower portion and an upper portion above the lower portion, and at least one conduit having one end in communication with the lower portion and another end in communication with the upper portion, and further comprising circulating the combined lead oxide and medium through the conduit while subjecting the combined lead oxide and medium to ultrasonic waves. 
     
     
       5. The method of claim 4, wherein the flask is immersed in a water bath, and further comprising cooling the conduit and thereby cooling the combined lead oxide and medium with the water bath while subjecting the combined lead oxide and medium to ultrasonic waves. 
     
     
       6. The method of claim 5, wherein the water bath is contained in a container, and further comprising flowing water through the container while subjecting the combined lead oxide and medium to ultrasonic waves. 
     
     
       7. The method of claim 4, wherein the circulation of the combined lead oxide and medium through the conduit is from the end in communication with the lower portion to the end in communication with the upper portion. 
     
     
       8. The method of claim 1, wherein the β-diketonate includes Pb(fod) 2  and the medium includes H-fod. 
     
     
       9. the method of claim 1, wherein the β-diketonate includes Pb(thd) 2  and the medium includes H-thd. 
     
     
       10. The method of claim 1, wherein the medium includes pentane.